Process of obtaining spirits of turpentine from wood.



PATENTED FEB. '7, 1905.

. J. C. MALLONBE. PROGESS 0I' OBTAINING SPIRITS 0F TURPENTINE PROM WOOD.

APPLICATION FILED 13110.23, 1903.

I ZSHEETS-SHBBT 1.

WWI/Loewe:

@AK/MMM@ J. G. MALLONEE.

lPATENIED PEB. 7, 1905.

PROCESS OF OBTAINING SPIRITS OP TURPENTINE FROM WOOD.

v APPLICATION FILED DEO. 23, 1903.

2 SHEETS-SHEET 2.

Ww i@ attoznms UNITED STATES Patented February 7, 1905.y

PATENT OFFICE. l .v

JOHN OAPLES MALLONEE, OF CHARLOTTE, NORTH CAROLINA.

PROCESS OF OBTAINING SPIRITS OF TURPENTINE FROM WOOD.

SPECIFICATION forming` part of Letters Patent No. '7B-1,733, dated February 7, 1905.

Application filed December 28, 1903. Serial No. 186,307.

To all whom it may concern:

Be it known that LJOHN CAPLES MALLONEE, a citizen of the United States, residing at Charlotte, in the county of Mecklenburg and State 5 of North Carolina, have invented new and useful Improvements in Processes of Obtaining Spirits of Turpentine from Wood, of which the following is a specification.

This invention has relation to the art or l process of obtaining spirits of turpentine and cognate substances from their woods, such as yellow pine; and it is the object constituting the invention to not only render the process more eicient and simple than heretofore, but

I to economize in substantially all of the steps necessary in the process, obviating a number of acts heretofore deemed necessary and substituting new steps which seem to me now to be of very great efficiency and importance.

2O To these ends my invention consists of the improvements which I will now proceed to describe in detail, explaining one of the means that I find suitable for carrying the invention into effect, and subsequently point out the in- :5 vention specifically in the claims hereto attached.

Of the drawings embodying the beforementioned means,Figure 1 is a side'elevation, parts being represented as broken away, of

.O the so-called first still and some of the connecting parts. Fig. 2 is a similar'view of the so-called second still. Fig. 3 is a crosssectional view of one of the stirrer or mixer arms, showing the Location of a perforated 5 steam-pipe located thereo`n. Fig. 4 is adiagrammatic View of a common still hereinafter referred to, parts being represented as broken away for the sake of clearness. Fig. 5 is an end view, partly in section, of the central holo low shaft and means for attaching the mixer e blades or arms to the shaft and showing also.` Fig.'

some important details of construction. 6 is an end view, partially in section, showing some details of construction in connection 5 with the mixer-arms, &c.A

Similar indicating numerals or marks indicate the same parts or features, as the case may be, throughout.

Heretofore the process generally employed O for securing turpentine and other oils or usef ful substances from pine wood has been car ried on in steel retorts by reducing the wood to charcoal under high temperatures, and, in short, by the process known as destructive distillation, the necessary apparatus employed 5 5 being very costly and short-li\fed,owing to the high temperatures employedin its operation. By my new process I carry on the operation under low-temperature conditions incident to the use of steam at ordinary boiler-pressures.

Before describing a form of apparatus that I may employ I will give a brief descriptionl of the process and some of the reasons for its use by me.

'Itis well known that such substances as creo- 65 sote and phenol oils do not exist in pine woods in a state of nature, but are produced in the retort during the decomposition of the wood by the high temperature employed. On the other hand, the resinous or fatty bodies native to the Wood separate into turpentinc and rosin at about the temperature or a little higher than boiling water. In the old method of destructive distillation as long as the water contained in the wood was being drivenof in the form of steam the turpentine was carried over and condensed in the coil, and the rosin was at the same time drawn out of the wood and fell or dripped to the bottom of the retort. This first flow of turpentine-oil was in the form of almost pure spirits, but was soon contaminated by the heavier oil produced, this latter phase being induced by the diiiiculty had i'i causing the steam to penetrate and be emitted from the pores of the wood in bulk. It is also well known that' even the highest grade of oils produced from pine wood under the process of destructive distillation are liable to be decomposed into inferior *and heavier bodies by contact with too high heats, and hence in'order to guard againstl this loss, which was constantly occurring, has been one of the designs or purposes of my new process, which,- as before stated, is operated under relatively low temperatures ex- 95 clusively. As experience has shown that it is due to the inability of the steam and low heat to penetrate the pores of the wood without raising the latter to a dangerous degree of heat, I have conceived the idea of disintegrat- IOC ing or debrating the wood and then subjecting each disintegrant or individual liber tota thorough steaming with a view of extracting the turpentine and rosin of merchantable purity and odor and in large quantities. In my experiments and practice I have found that simple ebullition or boiling of the water carried into the retort with the defibrated wood in filling thi` retort and steaming such mass while it is in a substantially still or quiet condition in the retort does not raise or volatilize certain oils sought after in the mass under treatment at the beginning of distillation with suiiicient thoroughness and rapidity to carry them over and prevent their decompol sition into or contamination by inferior and heavier bodies, but that in order to fully secure the oils sought after intheir purity it is necessary to agitate the mass in such manner as that the tendency will be to raise portions of the mass below toward the top and raise other portions below to the top, plunging top portions to or toward the bottom, and while this agitation is proceeding to constantly add live steam to the mass.

I need not here give a description of my method of reducing the wood to a` fibrous condition, as this can be done by any of the known ways of reducing wood to a chippy, pulpy, or fibrous condition suitable for treatment; but I will describe means which may be employed in carrying out the process forming the subject-matter of case.

In the initial` or first step or steps of the means shown for carrying my improvements into eect I use a still 1, built in the form of a cylinder, of any desired capacity, having a hollow steel shaft 2 running through it and journaled in stufling-boxes 3. This shaft carries a number of stout stirrer or mixer anms or blades 4, secured rigidly to it by means of intermediate cast-iron collars 5 working on a feather and fastened by set-screws 6, the shaft and attached arms being revolved by bevelgearing 7, of well-known construction, operated from any suitable prime motor.

The stirrer or agitating arms are groovcd in their rear edges upward, as at 8, for the reception of the perforated pipes 9, extended therein. the said pipes 9 being connected with pipes 10 by couplings 11, which connect the pipes 9 and 10, the latter connecting with the hollow of the steel shaft 2, (see particularly Figs. 3 and 4,) this construction and arrangement of parts being provided for the purpose of admitting steam from the hollow of the shaft 2 into the perforated pipes 9 and to cause said steam to commingle with the mass of fiber or pulp under treatment as the beater or stirrer arms are revolved. The pipe 12, carrying steam into the hollow shaft, receives steam from the engine-boiler andis attached to the central hollow shaft by means of a stationary stuffing-box 13, clamped rigidly to the pipe by thc stuiing-box 13, suitably packed and l it may contain.

lubricated, so that the shaft and stuving-box 13 may move while the pipe 12 remains stationary.

At the top of the still 1 is a vapor-pipe 14, connecting with an ordinary coil-condenser 15, and at the bottom the still, provided with a large draw-off gate 16 and a suitably large manhole-opening 17, is formed in the top for filling the still with p ulp.

The action of the, still is as follows: The shaft 2 being set in motion, the pulp or detibered wood is fed in through the manhole 17 by any suitable means, some water being run in at the same time to render the movement of the pulp and the mixers more easy. As soon as the still is filled the top opening or manhole 17 is closed, when steam is turned into the closed steam-coil 18, arranged in the bottom of the still. When the mass becomes thoroughly hot, which can be ascertained from feeling the vapor-pipe 14 with the hand or in any other suitablesway, live steam is turned into the hollow shaft by opening the gate or valve 19, with the double effect of aiding in the agitation of the pulp and at the same time bringing over into the vapor-pipe 14 the turpentine, which appears at this point somewhat discolored, necessitating further refining by simple distillation. The agitation of the mass under treatment, substantially as described, at the same time constantly adding live steam, is an important feature of the invention, since it effects a quicker and more thorough distillation of the oils first obtainable and preserves them for a longer time from the beginning of distillation against contamination by the heavier oils than could be otherwise the case, even with the deiibration of the wood. As soon,

as the iiow of turpentine ceases at the worm steam is shut ofi' from the hollow shaft, the hollow shaft is stopped, but the How of steam is maintained through the closed coil 18 in'the bottom of the still for some time longer or until it is judged that the rosin has collected well on the bottom ifi a uid state, at which time it is drawn off from the draw-off gate 16 somewhat mixed with pulp, but capable of being worked for rosin-oils or strained out as alow-grade commercial rosin. r1 .`he pulp after the rosin has been taken out is then run into a still 19, whichI call a digesterf where it is now treated to aweak solution of caustic soda or potash and where it is subjected to apressure varying from sixty to one hundred pounds, this being for the purpose of preventing the foaming over of the soapy liquid into the still and at the same time of driving into the fiber the soda solution with aview of leaching out what further resonance matters The excess of pressure is fed through aA regulating-valve into an ordinary condenser, and, as before said, it has been found that it prevents the foaming over of the soapy liquid into the still. Moreover, I have found that by carrying relatively high IOf IIC

IIC

,not contain any more turpentine-the still is gradually shut, pressure being blown off slowly and the contents discharged. The wood is now in a iinely-divided state and can be used for a variety of purposes-as,v for instance, paper-making, briqueting for kin' dling-blocks, or reduced to charcoal in the form of bricks, &c.

The oil resulting from this process is dark in color, but with apleasant turpentine andl pinene odor, and can readily be rendered water-white by simple distillation in any ordinary still, the final product being in no manner different from ordinary commercial spirits of good quality.

lt is to be distinctly understood that I have not shown nor described all of the ways in which an apparatus may be constructed or used for carrying into elect my improvements in the art of producing turpentine, rosinand their cognate ingredients from pine wood, since it is obvious that these may be varied, and, moreover, do not form any substantial part of my present invention.' Indeed, I have conceived of other means than those shown and which from continued practical experience now seem quite as valuable as those herein disclosed and may form subjects of separate applications. Furthermore, I do not bind myself to the precise manner of procedure which the use of some words here would imply. For example, in speaking of "(lelibrating or disintegrating wood I do not mean to be understood as binding myself to performing this act absolutely o r in the confined sense of the words employed, but defibratng or disintegrating thewood so as to separate it into its integrant particles to a degree or extent only that will enable me to carry out fairly the nature' and spirit of my invention.

What I claim is 1. The ar-t of extracting turpentine and its cognate substances from wood, `which consists in confining the mass under treatment, agitat vbelow to the top, plunging top portions to or .toward the bottom, and at the same time subjecting the mass throughout its entire body to steam at a relatively low temperature.

2. The art of extracting turpentine and its cognate substances from wood, which consists in confining the mass under treatment, subjecting it to heat and steam at a temperature of somewhat above 212O,agitatingit mechanically throughout its entire body in such manner that its tendency will be to raise, with certainty, portions of the mass below toward the top and raise other portions below tothe top, plunging top portions to or toward the bottom, and at the same time subjecting the mass throughout its entire body to steam and at a relatively low temperature.

3. The art of extracting turpentine, rosin and their cognate substances from wood sepa-ly rated into substantially its integrant fibers,

which consists in confining the mass to be treated and subjecting it to heat and steam at a relatively low temperature, thoroughly agitating the mass, substantially as described,

during this operation andconstantly adding live steam, then removing the rosin and-sub- -v jecting the mass to pressure varying between sixty and one hundred pounds.

4. 'Ihe art of extracting turpentine, rosin' and their cognate substances from wood which consists in rst deiibrating the wood, as described, and thendistilling it by means of steam applied to and permeating the entire mass, then removing the resinous substance and treating the pulp to a weak solution of.

caustic soda or potash, and finally treating it to heat and pressure varying from slxty to one hundred pounds.

In testimony whereof I have signed my name Witnesses:

E. R. COOPER, B. F. JORDAN.

`to this specification in the presence of two subl 

